HRID2368778
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Stannous chloride dihydrate (3.6 g, 16 mmol) was dissolved in 10 mL of concentrated hydrochloric acid. The solution was added to N-(2-methyl-5-nitrophenyl)-4,5′-bipyrimidin-2-amine with violent stirring. The mixture was poured into ice-cold water after being stirred for 2 hours. It was then neutralized to pH>8 with sodium carbonate and extracted with ethyl acetate for 4 times. The pooled extracts were washed with brine, dried over magnesium sulfate and finally concentrated under reduced pressure to obtain 0.7 g of the title compound. MS (M+1)=279.13.
WORKUP
后处理
- additionThe mixture was poured into ice-cold water
- extractionextracted with ethyl acetate for 4 times
- washThe pooled extracts were washed with brine
- dry with materialdried over magnesium sulfate
- concentrationfinally concentrated under reduced pressure